CN116283317B - Sagger for sintering sodium ion battery anode material and preparation method thereof - Google Patents
Sagger for sintering sodium ion battery anode material and preparation method thereof Download PDFInfo
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- CN116283317B CN116283317B CN202310218925.2A CN202310218925A CN116283317B CN 116283317 B CN116283317 B CN 116283317B CN 202310218925 A CN202310218925 A CN 202310218925A CN 116283317 B CN116283317 B CN 116283317B
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- sagger
- ion battery
- sintering
- sodium ion
- magnesia
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- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 229910001415 sodium ion Inorganic materials 0.000 title claims abstract description 50
- 238000005245 sintering Methods 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000010405 anode material Substances 0.000 title claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 65
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 43
- 239000011029 spinel Substances 0.000 claims abstract description 43
- 239000002245 particle Substances 0.000 claims abstract description 37
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000007774 positive electrode material Substances 0.000 claims abstract description 35
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 18
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 17
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 17
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 17
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 16
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims abstract description 16
- 229910052939 potassium sulfate Inorganic materials 0.000 claims abstract description 16
- 235000011151 potassium sulphates Nutrition 0.000 claims abstract description 16
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 16
- 239000004576 sand Substances 0.000 claims abstract description 15
- 229910021538 borax Inorganic materials 0.000 claims abstract description 14
- 239000004328 sodium tetraborate Substances 0.000 claims abstract description 14
- 235000010339 sodium tetraborate Nutrition 0.000 claims abstract description 14
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000465 moulding Methods 0.000 claims abstract description 11
- 238000007789 sealing Methods 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 6
- 239000000395 magnesium oxide Substances 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 11
- 239000011777 magnesium Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- QRNPTSGPQSOPQK-UHFFFAOYSA-N magnesium zirconium Chemical compound [Mg].[Zr] QRNPTSGPQSOPQK-UHFFFAOYSA-N 0.000 claims description 4
- -1 magnesium aluminate Chemical class 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 13
- 230000003628 erosive effect Effects 0.000 abstract description 12
- 230000035939 shock Effects 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 22
- 239000011734 sodium Substances 0.000 description 9
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 7
- 229910052708 sodium Inorganic materials 0.000 description 7
- 239000002994 raw material Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 239000002893 slag Substances 0.000 description 5
- 239000010406 cathode material Substances 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 230000018109 developmental process Effects 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 229910052863 mullite Inorganic materials 0.000 description 4
- 238000013112 stability test Methods 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 229920001353 Dextrin Polymers 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- 229910013716 LiNi Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 229910052664 nepheline Inorganic materials 0.000 description 1
- 239000010434 nepheline Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
-
- C—CHEMISTRY; METALLURGY
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
- C04B35/443—Magnesium aluminate spinel
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D5/00—Supports, screens, or the like for the charge within the furnace
- F27D5/0068—Containers
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
- C04B2235/3248—Zirconates or hafnates, e.g. zircon
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3409—Boron oxide, borates, boric acids, or oxide forming salts thereof, e.g. borax
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/442—Carbonates
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- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/444—Halide containing anions, e.g. bromide, iodate, chlorite
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/6567—Treatment time
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a sagger for sintering a positive electrode material of a sodium ion battery and a preparation method thereof. The preparation method comprises the following steps: s1, mixing magnesia-alumina spinel particles, magnesia-alumina spinel fine powder, magnesia-zirconia sand fine powder and borax according to a certain mass ratio to obtain a mixture; s2, dispersing and mixing ammonium bicarbonate solution, magnesium chloride solution, potassium sulfate solution and titanium tetrachloride solution in a certain mass ratio to obtain a mixed solution; s3, mixing the mixture and the mixed solution according to a certain mass ratio, and sealing and ageing to obtain a green body; s4, after the green body obtained in the step S3 is subjected to machine press molding, drying for a period of time at a certain temperature, and then carrying out high-temperature heat treatment for a period of time to obtain the sagger for sintering the positive electrode material of the sodium ion battery; wherein, steps S1 and S2 are not sequential. The preparation method provided by the invention has the advantages of simple process and low production cost, and the sagger for sintering the sodium ion battery anode material prepared by the method has the advantages of good sintering performance, high yield, strong erosion resistance and high thermal shock stability.
Description
Technical Field
The invention relates to the technical field of sodium ion batteries, in particular to a sagger for sintering a positive electrode material of a sodium ion battery and a preparation method thereof.
Background
The sodium ion battery is an important component in new energy batteries, and can be applied to the fields of energy storage, consumption, power and the like (Fang Xuezhou, lv Jingwen, zheng Tao, and the like; the current research situation of a positive electrode material of the sodium ion battery [ J ]. Battery, 2021, 51 (2): 201-204). The positive electrode material of the sodium ion battery is a key factor influencing the performance of the sodium ion battery, and the cost ratio is highest (Ding Yuyin, zhou Penghao, liu Jixin, and the like; the research on the positive electrode material and the negative electrode material of the sodium ion battery is advanced [ J ]. Chemical engineering, 2022, 30 (1): 57-62). Since commercial mass production of sodium ion batteries, saggers containing sodium ion battery anode materials have also received great attention.
Unlike lithium ion battery cathode materials, sodium ion battery cathode materials are more alkaline, and corrosion and penetration of the sagger by low viscosity sodium ion battery cathode precursors are exacerbated in high temperature solid phase processes, which results in a significant reduction in the service life of the sagger (Wang Yingnan, sun Hui. Study of the cathode material sintering process to produce sagger crystallization [ J. ]. Power technology, 2022, 46 (11): 1249-1252).
At present, few reports are reported on the development of a sagger for sintering a sodium ion battery anode material, and a material system of the sagger for sintering a lithium ion battery anode material, namely a composite material formed by cordierite-mullite/spinel is mainly adopted (Pengtao, liu Mingyang, zhou Wenying, and the like, and the magnesia-alumina spinel is used for calcining LiNi x Co y Mn z O 2 Impact of sagger material property for cathode material [ J]Refractory material, 2021, 55 (2): 102-106), the cordierite-mullite/spinel sagger still faces a plurality of problems in the heat treatment process of the sodium ion battery anode material, and the problems are mainly expressed in the following aspects:
(1) The corrosion of sodium source (sodium carbonate or sodium hydroxide) in the precursor of the positive electrode material of the sodium ion battery to the sagger is more serious, and the precursor is very easy to be matched with the acidic SiO in the sagger body 2 The components react to form natrium nepheline, and in the high-temperature (800-1000 ℃) heat treatment process of the positive electrode material of the sodium ion battery, the reaction is inevitably and continuously carried out, and the volume expansion of approximately 30-40% is initiated, so that the sagger is cracked and damaged.
(2) The sodium ion battery anode material has low viscosity, is molten at high temperature to form a liquid state, has stronger permeability to a cordierite-mullite/spinel sagger, and even directly penetrates through the side wall and the bottom of the sagger to cause the loss of the sodium ion battery anode material.
(3) During the reciprocating service process of the sagger for sintering the sodium electric positive electrode material, the cordierite-mullite/spinel sagger simultaneously faces the damage of cyclic thermal stress to cause the structural peeling of the sagger, so that the positive electrode material is polluted on one hand, and the purity and electrochemical performance of the sodium electric positive electrode material are affected; on the other hand, the damage of the sagger is accelerated.
(4) The sodium source in the sodium-electricity positive electrode material has high chemical reactivity, and is easy to be combined with other free components such as free Al in the heat treatment process 2 O 3 (f-Al 2 O 3 ) Free SiO 2 (f-SiO 2 ) The reaction forms high expansion phases such as sodium metaaluminate or sodium metasilicate/sodium silicate, etc., and accelerates cracking, peeling and damage of the sagger.
(5) The bonding system of the sagger is also an important factor affecting the service performance. The sagger belongs to a shaped sintered product, and has certain green strength to ensure the integral appearance of the baking and dehydrating stage and good sintering strength of a finished product. The traditional binding system (such as dextrin and the like) escapes in the sagger sintering process, pores are left, the density of the sagger is reduced, and the erosion resistance of the sagger is damaged; while strong acid binders (e.g., phosphoric acid, phosphates, etc.) are not volatile during the high temperature firing stage, but readily react with alkaline sodium sources to form a low melting phase. Salt-containing binders (such as pulp waste liquid and the like) are difficult to provide good early strength for the sagger, so that the sagger is cracked and damaged after being formed, and the rejection rate of the sagger is increased.
Disclosure of Invention
The invention aims at overcoming the defects of the prior art, and provides the preparation method of the sagger for sintering the sodium ion battery anode material, which has the advantages of simple process and low production cost.
The invention discloses a preparation method of a sagger for sintering a positive electrode material of a sodium ion battery, which comprises the following steps:
s1, mixing magnesia-alumina spinel particles, magnesia-alumina spinel fine powder, magnesia-zirconia sand fine powder and borax according to a certain mass ratio to obtain a mixture;
s2, dispersing and mixing ammonium bicarbonate solution, magnesium chloride solution, potassium sulfate solution and titanium tetrachloride solution in a certain mass ratio to obtain a mixed solution;
s3, mixing the mixture obtained in the step S1 and the mixed solution obtained in the step S2 according to a certain mass ratio, and sealing and placing to obtain a green body;
s4, after the green body obtained in the step S3 is subjected to machine press molding, drying for a period of time at a certain temperature, and then carrying out high-temperature heat treatment for a period of time to obtain the sagger for sintering the positive electrode material of the sodium ion battery;
wherein, steps S1 and S2 are not sequential.
In the step S1, the mass ratio of the magnesia-alumina spinel particles to the magnesia-alumina spinel fine powder to the magnesia-zirconia sand fine powder to the borax is 100:40-45:8-15:6-12.
Further, in the step S2, the mass ratio of the ammonium bicarbonate solution to the magnesium chloride solution to the potassium sulfate solution to the titanium tetrachloride solution is 100:50-80:40-70:20-30; wherein the concentration of the ammonium bicarbonate solution is 3-5 mol/L; the concentration of the magnesium chloride solution is 2-3 mol/L; the concentration of the potassium sulfate solution is 3-4 mol/L; the concentration of the titanium tetrachloride solution is 1-3 mol/L.
In step S2, the mixture is obtained by ultrasonic dispersion for 10 to 15 minutes under the water bath heating condition of 60 to 70 ℃.
Further, in the step S3, the mixed solution accounts for 5-7wt% of the mixed material; stirring for 15-20 min, sealing and ageing for 6-8 hr.
In step S4, the molding pressure is 60-80 MPa, the drying temperature is 110-120 ℃, the drying time is 4-8 hours, the heat treatment temperature is 1200-1250 ℃, and the drying time is 3-6 hours.
Further, the granularity of the magnesia-alumina spinel particles is 0.2-2.5 mm, wherein the particle sizes are respectively [0.2mm,0.5mm ], [0.5mm,1.2 mm) ], [1.2mm,1.8mm ], [1.8mm,2.5 mm), and the mass ratio of the particles is 100:25-40:15-18:5-8; al of the magnesia-alumina spinel particles 2 O 3 The content is 55-60 wt% and the MgO content is 38-40 wt%.
Further, the granularity of the magnesia-alumina spinel fine powder is 70-80 mu m; al of the magnesium aluminate spinel fine powder 2 O 3 The content is 70-78 wt% and the MgO content is 20-22 wt%.
Further, the granularity of the magnesium zirconium sand fine powder is 40-60 mu m; the MgO content of the magnesium zirconium sand fine powder is 88-90 wt percent, and ZrO 2 The content is 8-10wt%.
Further, the borax is industrially pure.
The sagger for sintering the positive electrode material of the sodium ion battery prepared by the preparation method.
By adopting the technical scheme, compared with the prior art, the invention has the following positive effects:
1. the raw materials selected by the invention are common components in the field of inorganic materials, the raw materials are wide in sources, no special equipment or technical requirements are required, the raw materials are only required to be uniformly mixed according to the proportion and then pressed, dried and sintered, the process is simple, and the method is suitable for industrial production of sagger.
2. The invention uses soluble titanium salt, magnesium salt and potassium salt components to form a precursor through ion exchange in ammonium bicarbonate buffer solution, and takes a magnesium source as a matrix in the high-temperature heat treatment process after the precursor is fully contacted with the mixture, so that abundant whiskers are formed in situ in the matrix, the structural toughness of the sagger matrix is enhanced, and the thermal shock stability of the sagger is improved.
3. The invention strengthens the combination of aggregate particles and matrix fine powder by the in-situ growth of the whisker, increases the roughness of the sagger by the staggered network structure and morphology, utilizes the alkaline components (magnesium and potassium) of the whisker to form isolation with the alkaline sodium ion battery anode material, improves the inertia of interface reaction and prevents the corrosion and penetration of the sodium ion battery anode material.
4. The invention is hydrolyzed by borax B (OH) 4 – And the hydroxyl group long chain links to form chemical combination, so that good early strength is provided for the sagger, the rate of finished products of the sagger products is improved, the sagger products are not decomposed and volatilized in the high-temperature treatment process, the density of the sagger is not reduced, ceramic phase compact combination can be formed, meanwhile, the alkalinity of a sagger material system is increased, and the erosion resistance of the sagger is further improved.
5. The raw material components of the invention have no f-Al 2 O 3 Or acidic SiO 2 And the components and the like, and the chemical reaction of an alkaline sodium source and a sagger in the positive electrode material of the sodium ion battery is avoided. In addition, the magnesia-alumina spinel and the magnesia-zirconia component raw materials have low thermal expansion coefficient and poor wettability with the sodium-electricity positive electrode material, so that the erosion resistance of the sagger is improved from the material design source, and the structural stability and the erosion resistance of the sagger are improvedSpalling properties.
6. According to the invention, close packing is formed by the grain composition of the raw material components and the critical grain size difference, and a liquid phase medium is provided by utilizing the combination of borax, so that the in-situ growth and development of whiskers and the sintering of the sagger are promoted, the sintering temperature of the sagger is obviously reduced, and the energy conservation and the environmental protection of the sagger development are facilitated.
The sagger for sintering the positive electrode material of the sodium ion battery prepared by the invention is used for detecting: the yield is 95-98%, and the volume density is 2.68-2.76 g/cm 3 The retention rate of residual flexural strength of the heat shock stability test at 1100 ℃ for 5 times is 88-92%, and the erosion index of the slag resistance test by a static crucible method at 1000 ℃ for 10 hours is 1.2-1.6%.
Therefore, the invention has the characteristics of simple process and low production cost, and the prepared sagger for sintering the sodium ion battery anode material has good sintering performance, high yield, strong erosion resistance and high thermal shock stability.
Drawings
FIG. 1 is an SEM photograph of the microstructure of a sagger prepared in example 2;
FIG. 2 is a diagram showing the Mg-B-O binary phase equilibrium;
FIG. 3 shows the sagger system Na resistance 2 The Factmage thermodynamics of the O erosion reaction.
Detailed Description
The following are specific embodiments of the present invention and the technical solutions of the present invention will be further described with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
Example 1
The preparation method of the sagger for sintering the positive electrode material of the sodium ion battery comprises the following steps:
s1, mixing magnesia-alumina spinel particles, magnesia-alumina spinel fine powder, magnesia-zirconia sand fine powder and borax according to a certain mass ratio to obtain a mixture;
s2, dispersing and mixing ammonium bicarbonate solution, magnesium chloride solution, potassium sulfate solution and titanium tetrachloride solution in a certain mass ratio to obtain a mixed solution;
s3, mixing the mixture obtained in the step S1 and the mixed solution obtained in the step S2 according to a certain mass ratio, and sealing and placing to obtain a green body;
s4, after the green body obtained in the step S3 is subjected to machine press molding, drying for a period of time at a certain temperature, and then carrying out high-temperature heat treatment for a period of time to obtain the sagger for sintering the positive electrode material of the sodium ion battery;
wherein, steps S1 and S2 are not sequential.
In the step S1, the mass ratio of the magnesia-alumina spinel particles, the magnesia-alumina spinel fine powder, the magnesia-zirconia sand fine powder and the borax is 100:42:13:8.
In the step S2, the mass ratio of the ammonium bicarbonate solution to the magnesium chloride solution to the potassium sulfate solution to the titanium tetrachloride solution is 100:65:45:22; wherein the concentration of the ammonium bicarbonate solution is 3mol/L; the concentration of the magnesium chloride solution is 3mol/L; the concentration of the potassium sulfate solution is 4mol/L; the concentration of the titanium tetrachloride solution is 2mol/L.
In the step S2, the mixture is obtained by ultrasonic dispersion for 15 minutes under the water bath heating condition of 65 ℃.
In the step S3, the mixed solution accounts for 5wt% of the mixed material; stirring for 20 min, and sealing and aging for 6 hr.
In the step S4, the pressure of the mechanical press molding is 65MPa, the drying temperature is 110 ℃, the drying time is 6 hours, the heat treatment temperature is 1230 ℃, and the time is 5 hours.
The particle size of the magnesia alumina spinel particles is 0.2-2.5 mm, wherein the mass ratio of the particles with the particle sizes of [0.2mm,0.5 mm), [0.5mm,1.2 mm), [1.2mm,1.8 mm) and [1.8mm,2.5 mm) is 100:28:16:6 respectively; al of the magnesia-alumina spinel particles 2 O 3 The content is 55-60 wt% and the MgO content is 38-40 wt%.
The sagger for sintering the positive electrode material of the sodium ion battery prepared in the embodiment detects: the yield was 96% and the bulk density was 2.72g/cm 3 The retention rate of residual flexural strength of the heat shock stability test at 1100 ℃ for 5 times is 91%, and the erosion index of the slag resistance test by a static crucible method at 1000 ℃ for 10 hours is 1.3%.
Example 2
The preparation method of the sagger for sintering the positive electrode material of the sodium ion battery comprises the following steps:
s1, mixing magnesia-alumina spinel particles, magnesia-alumina spinel fine powder, magnesia-zirconia sand fine powder and borax according to a certain mass ratio to obtain a mixture;
s2, dispersing and mixing ammonium bicarbonate solution, magnesium chloride solution, potassium sulfate solution and titanium tetrachloride solution in a certain mass ratio to obtain a mixed solution;
s3, mixing the mixture obtained in the step S1 and the mixed solution obtained in the step S2 according to a certain mass ratio, and sealing and placing to obtain a green body;
s4, after the green body obtained in the step S3 is subjected to machine press molding, drying for a period of time at a certain temperature, and then carrying out high-temperature heat treatment for a period of time to obtain the sagger for sintering the positive electrode material of the sodium ion battery;
wherein, steps S1 and S2 are not sequential.
In the step S1, the mass ratio of the magnesia-alumina spinel particles, the magnesia-alumina spinel fine powder, the magnesia-zirconia sand fine powder and the borax is 100:40:10:6.
In the step S2, the mass ratio of the ammonium bicarbonate solution to the magnesium chloride solution to the potassium sulfate solution to the titanium tetrachloride solution is 100:72:65:24; wherein the concentration of the ammonium bicarbonate solution is 4mol/L; the concentration of the magnesium chloride solution is 3mol/L; the concentration of the potassium sulfate solution is 3mol/L; the concentration of the titanium tetrachloride solution is 1mol/L.
In the step S2, the mixture is obtained by ultrasonic dispersion for 12 minutes under the condition of heating in a water bath at 70 ℃.
In the step S3, the mixed solution accounts for 6wt% of the mixed material; stirring for 18 min, and sealing and aging for 7 hr.
In the step S4, the pressure of the mechanical press molding is 60MPa, the drying temperature is 120 ℃, the drying time is 4 hours, the heat treatment temperature is 1220 ℃, and the time is 6 hours.
The particle size of the magnesia alumina spinel particles is 0.2-2.5 mm, wherein the mass ratio of the particles with the particle sizes of [0.2mm,0.5 mm), [0.5mm,1.2 mm), [1.2mm,1.8 mm) and [1.8mm,2.5 mm) is 100:35:18:8 respectively; al of the magnesia-alumina spinel particles 2 O 3 The content of the MgO is 55 to 60 percent by weight, and the MgO content is 38 to 40 percent by weight。
The sagger for sintering the positive electrode material of the sodium ion battery prepared in the embodiment detects: the yield is 98 percent, and the volume density is 2.68g/cm 3 The retention rate of residual flexural strength of the heat shock stability test at 1100 ℃ for 5 times is 89%, and the erosion index of the slag resistance test by a static crucible method at 1000 ℃ for 10 hours is 1.4%.
Example 3
The preparation method of the sagger for sintering the positive electrode material of the sodium ion battery comprises the following steps:
s1, mixing magnesia-alumina spinel particles, magnesia-alumina spinel fine powder, magnesia-zirconia sand fine powder and borax according to a certain mass ratio to obtain a mixture;
s2, dispersing and mixing ammonium bicarbonate solution, magnesium chloride solution, potassium sulfate solution and titanium tetrachloride solution in a certain mass ratio to obtain a mixed solution;
s3, mixing the mixture obtained in the step S1 and the mixed solution obtained in the step S2 according to a certain mass ratio, and sealing and placing to obtain a green body;
s4, after the green body obtained in the step S3 is subjected to machine press molding, drying for a period of time at a certain temperature, and then carrying out high-temperature heat treatment for a period of time to obtain the sagger for sintering the positive electrode material of the sodium ion battery;
wherein, steps S1 and S2 are not sequential.
In the step S1, the mass ratio of the magnesia-alumina spinel particles, the magnesia-alumina spinel fine powder, the magnesia-zirconia sand fine powder and the borax is 100:45:9:10.
In the step S2, the mass ratio of the ammonium bicarbonate solution to the magnesium chloride solution to the potassium sulfate solution to the titanium tetrachloride solution is 100:56:55:27; wherein the concentration of the ammonium bicarbonate solution is 3mol/L; the concentration of the magnesium chloride solution is 2mol/L; the concentration of the potassium sulfate solution is 4mol/L; the concentration of the titanium tetrachloride solution is 3mol/L.
In the step S2, the mixture is obtained by ultrasonic dispersion for 10 minutes under the condition of heating in a water bath at 70 ℃.
In the step S3, the mixed solution accounts for 7wt% of the mixed material; stirring for 15 min, and sealing and aging for 8 hr.
In the step S4, the pressure of the mechanical press molding is 80MPa, the drying temperature is 115 ℃, the drying time is 5 hours, the heat treatment temperature is 1200 ℃, and the time is 4 hours.
The particle size of the magnesia alumina spinel particles is 0.2-2.5 mm, wherein the mass ratio of the particles with the particle sizes of [0.2mm,0.5 mm), [0.5mm,1.2 mm), [1.2mm,1.8 mm) and [1.8mm,2.5 mm) is 100:25:17:7; al of the magnesia-alumina spinel particles 2 O 3 The content is 55-60 wt% and the MgO content is 38-40 wt%.
The sagger for sintering the positive electrode material of the sodium ion battery prepared in the embodiment detects: the yield was 97% and the bulk density was 2.75g/cm 3 The retention rate of the residual flexural strength of the heat shock stability test at 1100 ℃ for 5 times is 92%, and the erosion index of the slag resistance test by a static crucible method at 1000 ℃ for 10 hours is 1.2%.
FIG. 1 is an SEM photograph of the microstructure of a sagger prepared in example 2; from the figure, a large number of whiskers are formed in the sagger, the morphology of aggregate particles is kept good, and the whiskers mainly grow from a matrix and form a network structure in a staggered manner.
FIG. 2 is a diagram showing the Mg-B-O binary phase equilibrium; as can be seen from the figure, in the MgO-based material system B 2 O 3 The introduction of the whisker can provide a sufficient liquid medium environment and ensure the growth and development of the whisker.
FIG. 3 shows the sagger system Na resistance 2 As can be seen from the graph, the sagger material system has strong corrosion resistance, small formation amount of liquid phase (slag) and solid phase Mg 3 B 2 O 6 The formation of(s) together with the spinel solid phase(s) and the like effectively hinders erosion and penetration of the liquid phase melt.
The above is not relevant and is applicable to the prior art.
While certain specific embodiments of the present invention have been described in detail by way of example, it will be appreciated by those skilled in the art that the foregoing examples are provided for the purpose of illustration only and are not intended to limit the scope of the invention, and that various modifications or additions and substitutions to the described specific embodiments may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the invention as defined in the accompanying claims. It should be understood by those skilled in the art that any modification, equivalent substitution, improvement, etc. made to the above embodiments according to the technical substance of the present invention should be included in the scope of protection of the present invention.
Claims (10)
1. The preparation method of the sagger for sintering the anode material of the sodium ion battery is characterized by comprising the following steps of:
s1, mixing magnesia-alumina spinel particles, magnesia-alumina spinel fine powder, magnesia-zirconia sand fine powder and borax according to a certain mass ratio to obtain a mixture;
s2, dispersing and mixing ammonium bicarbonate solution, magnesium chloride solution, potassium sulfate solution and titanium tetrachloride solution in a certain mass ratio to obtain a mixed solution;
s3, mixing the mixture obtained in the step S1 and the mixed solution obtained in the step S2 according to a certain mass ratio, and sealing and placing to obtain a green body;
s4, after the green body obtained in the step S3 is subjected to machine press molding, drying for a period of time at a certain temperature, and then carrying out high-temperature heat treatment for a period of time to obtain the sagger for sintering the positive electrode material of the sodium ion battery;
wherein, steps S1 and S2 are not sequential.
2. The preparation method of the sagger for sintering the positive electrode material of the sodium ion battery according to claim 1, wherein in the step S1, the mass ratio of the magnesia-alumina spinel particles, the magnesia-alumina spinel fine powder, the magnesia-zirconia sand fine powder and the borax is 100: (40-45): (8-15): (6-12).
3. The preparation method of the sagger for sintering the positive electrode material of the sodium ion battery, which is characterized in that in the step S2, the mass ratio of the ammonium bicarbonate solution to the magnesium chloride solution to the potassium sulfate solution to the titanium tetrachloride solution is 100:50-80:40-70:20-30; wherein the concentration of the ammonium bicarbonate solution is 3-5 mol/L; the concentration of the magnesium chloride solution is 2-3 mol/L; the concentration of the potassium sulfate solution is 3-4 mol/L; the concentration of the titanium tetrachloride solution is 1-3 mol/L.
4. The method for preparing a sagger for sintering a positive electrode material of a sodium ion battery according to claim 1, wherein in the step S2, the mixed solution is obtained by ultrasonic dispersion for 10-15 minutes under the water bath heating condition of 60-70 ℃.
5. The method for preparing a sagger for sintering a positive electrode material of a sodium ion battery according to claim 1, wherein in the step S3, the mixed solution accounts for 5-7wt% of the mixed material; stirring for 15-20 min, sealing and ageing for 6-8 hr.
6. The method according to claim 1, wherein in the step S4, the molding pressure is 60 to 80MPa, the drying temperature is 110 to 120 ℃, the drying time is 4 to 8 hours, the heat treatment temperature is 1200 to 1250 ℃, and the time is 3 to 6 hours.
7. The preparation method of the sagger for sintering the positive electrode material of the sodium ion battery according to claim 1, wherein the particle size of the magnesia-alumina spinel particles is 0.2-2.5 mm, and the mass ratio of the particles with the particle sizes of [0.2mm,0.5mm ], [0.5mm,1.2mm ], [1.2mm,1.8mm ], [1.8mm,2.5 mm) is 100:25-40:15-18:5-8; al of the magnesia-alumina spinel particles 2 O 3 The content is 55-60 wt% and the MgO content is 38-40 wt%.
8. The method for preparing a sagger for sintering a positive electrode material of a sodium ion battery according to claim 1, wherein the granularity of the magnesia-alumina spinel fine powder is 70-80 μm; al of the magnesium aluminate spinel fine powder 2 O 3 The content is 70-78 wt% and the MgO content is 20-22 wt%.
9. According toThe method for preparing the sagger for sintering the anode material of the sodium ion battery, which is characterized in that the granularity of the magnesium zirconium sand fine powder is 40-60 mu m; the MgO content of the magnesium zirconium sand fine powder is 88-90 wt percent, and ZrO 2 The content is 8-10wt%.
10. A sagger for sintering a positive electrode material of a sodium ion battery prepared by the preparation method of any one of claims 1 to 9.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010015296A2 (en) * | 2008-08-06 | 2010-02-11 | Carl Zeiss Smt Ag | Transmitting optical element consisting of magnesium-aluminium spinel |
| CN102583585A (en) * | 2012-01-09 | 2012-07-18 | 安徽亚兰德新能源材料股份有限公司 | Preparation technology for spherical lithium cobalt oxide doped with Ti, Mg and Al |
| CN103601521A (en) * | 2013-11-15 | 2014-02-26 | 瑞泰科技股份有限公司 | Low-porosity periclase-magnesium aluminate spinel-zirconia sintered composite refractory material and production process thereof |
| CN104193368A (en) * | 2014-08-28 | 2014-12-10 | 洛阳利尔耐火材料有限公司 | Magnesium-spinel brick for RH (Rheinstahl-Hutlenwerke) refining furnaces and preparation method thereof |
| CN107285787A (en) * | 2017-07-28 | 2017-10-24 | 武汉科技大学 | A kind of lightweight corundum fireproof magnesia alumina spinel material and preparation method thereof |
| CN112279662A (en) * | 2020-11-06 | 2021-01-29 | 湘潭海泡石科技有限公司 | Sagger for magnesium aluminate spinel-cordierite calcined lithium battery positive electrode material and preparation method thereof |
| CN114230371A (en) * | 2021-11-26 | 2022-03-25 | 汉川市石金科技有限公司 | Composite coating for improving corrosion resistance of sagger surface and prolonging service life |
| WO2022105175A1 (en) * | 2020-11-19 | 2022-05-27 | 山东玉皇新能源科技有限公司 | Positive electrode material of sodium ion battery, preparation method therefor, and sodium ion battery |
| WO2022127314A1 (en) * | 2020-12-15 | 2022-06-23 | 广东邦普循环科技有限公司 | Saggar for sintering lithium transition metal oxide, and preparation method therefor |
-
2023
- 2023-03-08 CN CN202310218925.2A patent/CN116283317B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010015296A2 (en) * | 2008-08-06 | 2010-02-11 | Carl Zeiss Smt Ag | Transmitting optical element consisting of magnesium-aluminium spinel |
| CN102583585A (en) * | 2012-01-09 | 2012-07-18 | 安徽亚兰德新能源材料股份有限公司 | Preparation technology for spherical lithium cobalt oxide doped with Ti, Mg and Al |
| CN103601521A (en) * | 2013-11-15 | 2014-02-26 | 瑞泰科技股份有限公司 | Low-porosity periclase-magnesium aluminate spinel-zirconia sintered composite refractory material and production process thereof |
| CN104193368A (en) * | 2014-08-28 | 2014-12-10 | 洛阳利尔耐火材料有限公司 | Magnesium-spinel brick for RH (Rheinstahl-Hutlenwerke) refining furnaces and preparation method thereof |
| CN107285787A (en) * | 2017-07-28 | 2017-10-24 | 武汉科技大学 | A kind of lightweight corundum fireproof magnesia alumina spinel material and preparation method thereof |
| CN112279662A (en) * | 2020-11-06 | 2021-01-29 | 湘潭海泡石科技有限公司 | Sagger for magnesium aluminate spinel-cordierite calcined lithium battery positive electrode material and preparation method thereof |
| WO2022105175A1 (en) * | 2020-11-19 | 2022-05-27 | 山东玉皇新能源科技有限公司 | Positive electrode material of sodium ion battery, preparation method therefor, and sodium ion battery |
| WO2022127314A1 (en) * | 2020-12-15 | 2022-06-23 | 广东邦普循环科技有限公司 | Saggar for sintering lithium transition metal oxide, and preparation method therefor |
| CN114230371A (en) * | 2021-11-26 | 2022-03-25 | 汉川市石金科技有限公司 | Composite coating for improving corrosion resistance of sagger surface and prolonging service life |
Non-Patent Citations (1)
| Title |
|---|
| 锂电池正极材料合成用堇青石-莫来石质匣钵研究进展;段雪珂;王新福;刘国齐;王龙光;陈红伟;钱凡;;耐火材料(第02期);第27-31页 * |
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